We report the synthesis and characterization of two iridium polypyridyl complexes, [Ir(deeb)2Cl2](PF6) and [Ir(deeb)2(dpp)](PF6)3, where deeb = diethyl-2,2′-bipyridine-4,4′-dicarboxylate and dpp = 2,3-bis(2-pyridyl)pyrazine. From 1H NMR spectral data, the two deeb ligands are attached to Ir cis to each other. Mass spectra contain fragmentation patterns of the (M-PF6)+ and (M-3PF6)3+ molecular ions for [Ir(deeb)2Cl2](PF6) and [Ir(deeb)2(dpp)](PF6)3, respectively. The electronic absorption spectrum of [Ir(deeb)2Cl2](PF6) shows maxima at 308 nm and 402 nm, which are assigned as 1π → π* and metal-to-ligand charge transfer transitions, respectively. [Ir(deeb)2(dpp)](PF6)3 exhibits peaks due to 1π → π* transitions at 322 nm and 334 nm. [Ir(deeb)2Cl2](PF6) has emission peaks at 538 nm in acetonitrile and 567 nm in the solid state, with lifetimes of 1.71 µs and 0.35 µs, respectively. [Ir(deeb)2Cl2](PF6) has an unusually higher quantum yield than analogous compounds. [Ir(deeb)2(dpp)](PF6)3 has emission peaks at 540 nm in acetonitrile and 599 nm in the solid state with lifetimes of 1.23 µs and 0.14 µs, respectively. Cyclic voltammetry of [Ir(deeb)2Cl2](PF6) yields two reversible couples at −0.72 and −0.87 V versus Ag/AgCl, both corresponding to deeb ligand reductions, and a quasi-reversible couple at −1.48 V corresponding to Ir3+/+ reduction. Electrochemical reduction of [Ir(deeb)2(dpp)](PF6)3 yields couples at −0.38, −0.54, −0.71, and −1.33 V, assigned as deeb0/−, deeb0/−, dpp0/−, and Ir3+/+ reductions, respectively.